CN109209498B - Method for sealing coal mine underground long-distance fire area - Google Patents
Method for sealing coal mine underground long-distance fire area Download PDFInfo
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- CN109209498B CN109209498B CN201811180447.6A CN201811180447A CN109209498B CN 109209498 B CN109209498 B CN 109209498B CN 201811180447 A CN201811180447 A CN 201811180447A CN 109209498 B CN109209498 B CN 109209498B
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21F—SAFETY DEVICES, TRANSPORT, FILLING-UP, RESCUE, VENTILATION, OR DRAINING IN OR OF MINES OR TUNNELS
- E21F17/00—Methods or devices for use in mines or tunnels, not covered elsewhere
- E21F17/103—Dams, e.g. for ventilation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention discloses a method for sealing a remote fire area under a coal mine, which comprises the steps of carrying out directional drilling construction from an air inlet roadway and an air return roadway of a ground fire area working surface by using an accurate positioning drilling technology, and determining the construction position of a fire area sealing wall; respectively filling polymer filling materials into the drill holes of the air inlet lane and the air return lane through pipelines to form a sealing wall; the polymer filling material comprises a component A and a component B, wherein the component A comprises composite resin, aromatic polyamide fiber, polyvinylpyrrolidone, ethylene glycol, a composite flame retardant, triethylene diamine, dichloromethane, a composite foam stabilizer and polymethyl methacrylate; the component B is a compound of benzenesulfonic acid and dimethylolpropionic acid; the problems of long fire zone sealing time, large labor capacity, poor operation environment, construction safety and the like in the existing fire zone sealing process are solved, and the long-distance safe sealing of the fire zone is realized.
Description
Technical Field
The invention belongs to the field of coal mine fire control, and particularly relates to a method for sealing a long-distance fire area under a coal mine.
Background
Mine fire is one of main disasters of coal mines, and when a fire disaster occurs on a coal face, if a direct fire extinguishing method cannot effectively control the fire condition, the fire area is closed to prevent the fire area from further expanding or eliminate the influence of the fire area on an adjacent mining area, which is the most reliable fire prevention and extinguishing measure. At present, a sealing mode of an underground fire area of a coal mine is mainly formed by constructing an explosion-proof wall by sand bags and a sealing wall constructed by red bricks, a large amount of sand bags, red bricks, cement and other materials are needed in the sealing process of the fire area, underground transportation quantity and labor quantity are large, the sealing time of the fire area is long, and the optimal sealing time of the fire area is easy to miss. In addition, because coal spontaneous combustion fire generates a large amount of toxic and harmful gas and heat, the closed operation environment of a fire area is poor, particularly a high-gas mine, and in the closed process of the fire area, gas explosion accidents can be caused at any time due to gas accumulation, so that larger malignant accidents are caused.
Disclosure of Invention
In view of the above, the invention aims to provide a method for sealing a remote fire area in a coal mine, which solves the problems of long fire area sealing time, large labor capacity, poor operation environment, construction safety and the like in the existing fire area sealing process, and realizes remote safe sealing of the fire area.
The invention discloses a method for sealing a remote fire area under a coal mine, which is characterized by comprising the following steps: the method comprises the following steps: a. performing directional drilling construction from an air inlet roadway and an air return roadway of a ground fire zone working face by using an accurate positioning drilling technology, and determining a construction position of a fire zone sealing wall;
b. respectively filling polymer filling materials into the drill holes of the air inlet lane and the air return lane through pipelines to form a sealing wall;
the polymer filling material comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 15-25 parts of composite resin, 4-8 parts of aromatic polyamide fiber, 1-3 parts of polyvinylpyrrolidone, 1-3 parts of ethylene glycol, 5-10 parts of composite flame retardant, 3-7 parts of triethylene diamine, 10-15 parts of dichloromethane, 5-10 parts of composite foam stabilizer and 0.5-1 part of polymethyl methacrylate;
the composite resin is prepared from expandable phenolic resin and urea-formaldehyde resin according to the mass ratio of 2: 1, compounding; the composite flame retardant is prepared from dimethyl methyl phosphate: tris (1-chloro-2-propyl) phosphate: expanded graphite 12: 8: 15, compounding; the composite foam stabilizer is castor oil polyoxyethylene ether in mass ratio: tween-80 ═ 3: 1, compounding;
the component B comprises benzene sulfonic acid in a mass ratio: dimethylolpropionic acid ═ 2: 1, compounding;
further, in the step b, nitrogen is input as conveying power during filling, and pressure monitoring is carried out;
further, in the step B, the component A and the component B are conveyed to the bottom of a drilled hole according to the ratio of 4: 1-8: 1 and then mixed through a static mixer;
further, the pipeline comprises an A component conveying pipeline, a B component conveying pipeline and a nitrogen auxiliary pipeline which is respectively communicated with an inlet of the A component conveying pipeline and an inlet of the B component conveying pipeline, a pressure gauge is arranged on the nitrogen pipeline, and a flow meter, a flow control valve and a one-way valve are arranged on the A component conveying pipeline and the B component conveying pipeline;
further, outlets of the component A conveying pipeline and the component B conveying pipeline are arranged within 20cm of a closed roadway roof;
further, the preparation method of the expandable phenolic resin comprises the following steps: mixing phenol and 37 mass percent formaldehyde aqueous solution, heating to 35-45 ℃, slowly dripping 50 mass percent sodium hydroxide aqueous solution into the system under rapid stirring, controlling the temperature of the system to be not higher than 60 ℃, adjusting the water bath temperature to 45-55 ℃ after finishing dripping, reacting for 1-3 hours, then heating to 75-85 ℃ for reacting for 2-4 hours, after the reaction is finished, rapidly cooling the system to below 40 ℃ by cold water, adjusting the system to be neutral, and finally performing vacuum dehydration to proper viscosity at the temperature of 55-60 ℃;
further, the molar percentage of sodium hydroxide to phenol in the aqueous sodium hydroxide solution is 0.05: 1, the molar ratio of formaldehyde to phenol is 1.6-1.8: 1;
further, the expandable graphite is treated by:
1) mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with expandable graphite, and drying at 55-65 ℃ for 5-6 hours for later use;
2) mixing the dried 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in the step 1) with a silane coupling agent, and stirring in an oil bath at the temperature of 150-;
3) mixing the expandable graphite dried in the step 1) with deionized water, adjusting the pH value to 3-5, adding the product obtained in the step 2) and ethanol, stirring for 3.5-4.5 hours at the water bath temperature of 55-65 ℃, filtering, washing and drying the product at the temperature of 55-65 ℃ for 5-6 hours.
The invention has the beneficial effects that: the invention discloses a method for sealing a remote fire area under a coal mine, which selects a high polymer material consisting of two components as a remote fire area sealing material, wherein the material contains low free formaldehyde, has high resin activity, rapid solidification and high expansion performance, the formed foam has small density, the foaming expansion multiple is more than 35 times, the foam reaction speed is high, the reaction can be finished within 20-30s at normal temperature, the expansion is finished within 3-5min at 10-15 ℃, the foam is hardened within 15min, the foam has good flame retardance and combustion resistance, the foam can be actively connected, after slurry is injected into a filling space, the closed space including coal rock cracks at the periphery of a roadway is filled, the filling material is subjected to self expansion extrusion after the top of the closed wall is filled, a filling body is tightly combined with the periphery of the roadway, the fire area is shrunk and communicated with the closed area, and an insulating wall body with good integrity and gas sealing is formed, playing a good isolating role. By adopting the material and combining the plugging method, the purposes of short sealing time of a fire zone, labor amount reduction, working environment improvement of underground operators and construction safety improvement are achieved, the effects of large-area filling and grouting of a goaf and plugging and cooling can be realized, the impact kinetic energy of gas explosion can be absorbed, the impact resistance of the constructed airtight wall is strong, and the long-distance safe sealing of the fire zone is realized.
Detailed Description
The method for sealing the underground long-distance fire area of the coal mine comprises the following steps: a. performing directional drilling construction from an air inlet roadway and an air return roadway of a ground fire zone working face by using an accurate positioning drilling technology, and determining a construction position of a fire zone sealing wall;
b. respectively filling polymer filling materials into the drill holes of the air inlet lane and the air return lane through pipelines to form a sealing wall;
the polymer filling material comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 15-25 parts of composite resin, 4-8 parts of aromatic polyamide fiber, 1-3 parts of polyvinylpyrrolidone, 1-3 parts of ethylene glycol, 5-10 parts of composite flame retardant, 3-7 parts of triethylene diamine, 10-15 parts of dichloromethane, 5-10 parts of composite foam stabilizer and 0.5-1 part of polymethyl methacrylate;
the composite resin is prepared from expandable phenolic resin and urea-formaldehyde resin according to the mass ratio of 2: 1, compounding; the composite flame retardant is prepared from dimethyl methyl phosphate: tris (1-chloro-2-propyl) phosphate: expanded graphite 12: 8: 15, compounding; the composite foam stabilizer is castor oil polyoxyethylene ether in mass ratio: tween-80 ═ 3: 1, compounding;
the component B comprises benzene sulfonic acid in a mass ratio: dimethylolpropionic acid ═ 2: 1, compounding; the aromatic polyamide fiber is compounded with the phenolic resin and the urea-formaldehyde resin as main raw materials, wherein the aromatic polyamide fiber has good flame retardance, is non-combustible when meeting open fire and has good affinity with the phenolic resin, the phenolic resin can be effectively enhanced, the toughening effect is achieved through the synergistic effect of polyvinylpyrrolidone and glycol, the synergistic effect of dimethyl methyl phosphonate, tris (1-chloro-2-propyl) phosphate and expandable graphite is achieved, the synergistic effect of castor oil polyoxyethylene ether and tween-80 is achieved, fine and uniform foam is formed through the synergistic effect of the castor oil polyoxyethylene ether and the tween-80 and the other components, the foam density is small, the foaming multiple is improved, and the synergistic effect of benzenesulfonic acid and dimethylolpropionic acid is matched with the other components to achieve the characteristics of strong plasticization, stable foaming performance and fine and uniform foam. The components of the above components have an inseparable influence on the product performance, for example, the addition amount of the composite foam stabilizer is too small, the intersolubility between the components is low, the surface tension of the components is high, the foam is difficult to form or unstable, the foam is uneven, the closed cell rate is high, if the addition amount is excessive, the crosslinking curing reaction of the resin is influenced, the foaming speed and the curing speed are influenced, a large amount of foaming agent escapes from the resin in the form of bubbles, the foam quality is influenced, the foaming multiple is reduced, and similarly, the addition amount of the foaming agent in the material not only influences the expansion effect, but also obviously influences the compressive strength of the cured material after expansion. The colloid material is heated and then is heated integrally, so that the phenomena of volatilization of a large amount of water vapor and the like can be avoided, the toughness is good, the stratum movement can be borne, the impact resistance is high, and the compressive strength is more than 10KPa when the deformation of the colloid material is 10%. The material is suitable for long-distance mechanical operation, so that the threat of potential safety hazards of filling sealing points to operators is reduced, and the working environment of underground operators is improved.
In the embodiment, in the step b, nitrogen is input as conveying power during filling, and pressure monitoring is performed; and nitrogen is added at the inlets of the component A conveying pipeline and the component B conveying pipeline to serve as conveying power, the oxygen environment at the periphery of a fire area is inerted, the diffusion radius of the material is increased, and the diffusion range in a roadway reaches 3-5 m. The pressure gauge parameters can directly reflect the pipeline blockage and the top connection effect of the sealing wall.
In the embodiment, in the step B, the component A and the component B are conveyed to the bottom of a drilled hole according to the ratio of 4: 1-8: 1 and then mixed by a static mixer; the flow state of the two component materials in the pipe is continuously changed by using a static mixer at the bottom of a drilling hole, and A, B components are fully mixed according to the rule of 'segmentation-displacement-overlap'. Preferably, the ratio of the A component to the B component is 6:1, and the above ratio is a weight ratio.
In this embodiment, the pipeline includes A group's component conveying line and B group's component conveying line and communicates the imported nitrogen gas auxiliary line of A group's component conveying line import and B group's component conveying line import respectively, be provided with the manometer on the nitrogen gas pipeline, be provided with flowmeter and flow control valve and check valve on A group's component conveying line and the B group's component conveying line. The check valves are arranged at the tail ends of the component A conveying pipeline and the component B conveying pipeline, so that the pipeline blockage caused by material backflow is avoided. A. A flow control valve and a flowmeter are arranged on a grouting pipeline for the two materials of the component B to control the proportion of the two materials of the component A, B, and meanwhile, check valves are respectively arranged at the tail ends of the pipelines to avoid the phenomenon of backflow blockage of the pipeline by A, B slurry.
In the embodiment, outlets of the component A conveying pipeline and the component B conveying pipeline are arranged within 20cm of a closed roadway roof; the problem that the expansion filling material cannot realize material top sealing due to the blockage of a pipeline outlet is avoided.
In this embodiment, the preparation method of the expandable phenolic resin includes the following steps: mixing phenol and 37 mass percent formaldehyde aqueous solution, heating to 35-45 ℃, slowly dripping 50 mass percent sodium hydroxide aqueous solution into the system under rapid stirring, controlling the temperature of the system to be not higher than 60 ℃, adjusting the water bath temperature to 45-55 ℃ after finishing dripping, reacting for 1-3 hours, then heating to 75-85 ℃ for reacting for 2-4 hours, after the reaction is finished, rapidly cooling the system to below 40 ℃ by cold water, adjusting the system to be neutral, and finally performing vacuum dehydration to proper viscosity at the temperature of 55-60 ℃; the preparation method of the specific expandable phenolic resin improves the activity of the resin and reduces the generation of free formaldehyde.
In this embodiment, the mole percentage of sodium hydroxide to phenol in the sodium hydroxide aqueous solution is 0.05: 1, the molar ratio of formaldehyde to phenol is 1.6-1.8: 1;
in this example, the expandable graphite was treated by:
1) mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with expandable graphite, and drying at 55-65 ℃ for 5-6 hours for later use;
2) mixing the dried 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in the step 1) with a silane coupling agent, and stirring in an oil bath at the temperature of 150-;
3) mixing the expandable graphite dried in the step 1) with deionized water, adjusting the pH value to 3-5, adding the product obtained in the step 2) and ethanol, stirring for 3.5-4.5 hours at the water bath temperature of 55-65 ℃, filtering, washing and drying the product at the temperature of 55-65 ℃ for 5-6 hours.
Example one
The component A comprises the following raw materials in parts by weight: 15 parts of composite resin, 4 parts of aromatic polyamide fiber, 1 part of polyvinylpyrrolidone, 1 part of ethylene glycol, 5 parts of composite flame retardant, 3 parts of triethylene diamine, 10 parts of dichloromethane, 5 parts of composite foam stabilizer and 0.5 part of polymethyl methacrylate;
the preparation method of the expandable phenolic resin comprises the following steps: mixing phenol and 37 mass percent aqueous formaldehyde solution, heating to 35 ℃, slowly dripping 50 mass percent aqueous sodium hydroxide solution into the system under rapid stirring, controlling the temperature of the system to be not higher than 60 ℃, adjusting the water bath temperature to 45 ℃ after finishing dripping, reacting for 1 hour, then heating to 75 ℃ for 2 hours, after the reaction, rapidly cooling the system to below 40 ℃ by cold water, adjusting the system to be neutral, and finally dehydrating in vacuum to proper viscosity at the temperature of 55 ℃; wherein, the mole percentage of sodium hydroxide and phenol in the sodium hydroxide aqueous solution is 0.05: 1, the molar ratio of formaldehyde to phenol is 1.6: 1;
the expandable graphite is treated by:
1) mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with expandable graphite, and drying at 55 ℃ for 5 hours for later use;
2) mixing the dried 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in the step 1) with a silane coupling agent, and stirring in an oil bath for 3.5 hours at the temperature of 150 ℃;
3) mixing the expandable graphite dried in the step 1) with deionized water, adjusting the pH value to 3, adding the product obtained in the step 2) and ethanol, stirring for 3.5 hours at the water bath temperature of 55 ℃, performing suction filtration and washing on the product, and drying for 5 hours at the temperature of 55 ℃;
in the present example, the length of the aromatic polyamide fiber was 6 mm.
Example two
The component A comprises the following raw materials in parts by weight: 25 parts of composite resin, 8 parts of aromatic polyamide fiber, 3 parts of polyvinylpyrrolidone, 3 parts of ethylene glycol, 10 parts of composite flame retardant, 7 parts of triethylene diamine, 15 parts of dichloromethane, 10 parts of composite foam stabilizer and 1 part of polymethyl methacrylate;
the preparation method of the expandable phenolic resin comprises the following steps: mixing phenol and 37 mass percent aqueous formaldehyde solution, heating to 45 ℃, slowly dripping 50 mass percent aqueous sodium hydroxide solution into the system under rapid stirring, controlling the temperature of the system to be not higher than 60 ℃, adjusting the water bath temperature to 55 ℃ after the dripping is finished, reacting for 3 hours, then heating to 85 ℃ for reacting for 4 hours, after the reaction is finished, rapidly cooling the system to below 40 ℃ by using cold water, adjusting the system to be neutral, and finally performing vacuum dehydration to proper viscosity at the temperature of 60 ℃; wherein, the mole percentage of sodium hydroxide and phenol in the sodium hydroxide aqueous solution is 0.05: 1, the molar ratio of formaldehyde to phenol is 1.8: 1;
the expandable graphite is treated by:
1) mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with expandable graphite, and drying at 65 ℃ for 6 hours for later use;
2) mixing the dried 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in the step 1) with a silane coupling agent, and stirring in an oil bath for 4.5 hours at the temperature of 170 ℃;
3) mixing the expandable graphite dried in the step 1) with deionized water, adjusting the pH value to 5, then adding the product obtained in the step 2) and ethanol, stirring for 4.5 hours at the water bath temperature of 65 ℃, and drying the product at the temperature of 65 ℃ for 6 hours after carrying out suction filtration and washing;
in the present example, the length of the aromatic polyamide fiber was 10 mm.
EXAMPLE III
The component A comprises the following raw materials in parts by weight: 15 parts of composite resin, 8 parts of aromatic polyamide fiber, 1 part of polyvinylpyrrolidone, 3 parts of ethylene glycol, 5 parts of composite flame retardant, 7 parts of triethylene diamine, 10 parts of dichloromethane, 10 parts of composite foam stabilizer and 1 part of polymethyl methacrylate;
the preparation method of the expandable phenolic resin comprises the following steps: mixing phenol and 37 mass percent aqueous formaldehyde solution, heating to 35 ℃, slowly dripping 50 mass percent aqueous sodium hydroxide solution into the system under rapid stirring, controlling the temperature of the system to be not higher than 60 ℃, adjusting the water bath temperature to 55 ℃ after the dripping is finished, reacting for 1 hour, then heating to 85 ℃ for reacting for 2 hours, after the reaction is finished, rapidly cooling the system to below 40 ℃ by using cold water, adjusting the system to be neutral, and finally performing vacuum dehydration to proper viscosity at the temperature of 60 ℃; wherein, the mole percentage of sodium hydroxide and phenol in the sodium hydroxide aqueous solution is 0.05: 1, the molar ratio of formaldehyde to phenol is 1.6: 1;
the expandable graphite is treated by:
1) mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with expandable graphite, and drying at 65 ℃ for 5 hours for later use;
2) mixing the dried 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in the step 1) with a silane coupling agent, and stirring in an oil bath for 3.5 hours at the temperature of 170 ℃;
3) mixing the expandable graphite dried in the step 1) with deionized water, adjusting the pH value to 5, then adding the product obtained in the step 2) and ethanol, stirring for 4.5 hours at the water bath temperature of 55 ℃, and drying the product at the temperature of 55 ℃ for 6 hours after carrying out suction filtration and washing;
in the present example, the length of the aromatic polyamide fiber was 6 mm.
Example four
The component A comprises the following raw materials in parts by weight: 25 parts of composite resin, 4 parts of aromatic polyamide fiber, 3 parts of polyvinylpyrrolidone, 1 part of ethylene glycol, 10 parts of composite flame retardant, 3 parts of triethylene diamine, 15 parts of dichloromethane, 5 parts of composite foam stabilizer and 0.5 part of polymethyl methacrylate;
the preparation method of the expandable phenolic resin comprises the following steps: mixing phenol and 37 mass percent aqueous formaldehyde solution, heating to 45 ℃, slowly dripping 50 mass percent aqueous sodium hydroxide solution into the system under rapid stirring, controlling the temperature of the system to be not higher than 60 ℃, adjusting the water bath temperature to 45 ℃ after the dripping is finished, reacting for 3 hours, then heating to 75 ℃ for 4 hours, after the reaction is finished, rapidly cooling the system to below 40 ℃ by cold water, adjusting the system to be neutral, and finally dehydrating in vacuum to proper viscosity at the temperature of 55 ℃; wherein, the mole percentage of sodium hydroxide and phenol in the sodium hydroxide aqueous solution is 0.05: 1, the molar ratio of formaldehyde to phenol is 1.8: 1;
the expandable graphite is treated by:
1) mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with expandable graphite, and drying at 55 ℃ for 6 hours for later use;
2) mixing the dried 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in the step 1) with a silane coupling agent, and stirring in an oil bath for 4.5 hours at the temperature of 150 ℃;
3) mixing the expandable graphite dried in the step 1) with deionized water, adjusting the pH value to 3, then adding the product obtained in the step 2) and ethanol, stirring for 3.5 hours at the water bath temperature of 65 ℃, and drying the product for 5 hours at the temperature of 65 ℃ after carrying out suction filtration and washing;
in the present example, the length of the aromatic polyamide fiber was 7 mm.
EXAMPLE five
The component A comprises the following raw materials in parts by weight: 18 parts of composite resin, 4 parts of aromatic polyamide fiber, 2 parts of polyvinylpyrrolidone, 3 parts of ethylene glycol, 7 parts of composite flame retardant, 3 parts of triethylene diamine, 12 parts of dichloromethane, 10 parts of composite foam stabilizer and 0.5 part of polymethyl methacrylate;
the preparation method of the expandable phenolic resin comprises the following steps: mixing phenol and 37 mass percent aqueous formaldehyde solution, heating to 38 ℃, slowly dripping 50 mass percent aqueous sodium hydroxide solution into the system under rapid stirring, controlling the temperature of the system to be not higher than 60 ℃, adjusting the water bath temperature to 45 ℃ after finishing dripping, reacting for 2 hours, then heating to 78 ℃ for reacting for 3 hours, after the reaction is finished, rapidly cooling the system to below 40 ℃ by using cold water, adjusting the system to be neutral, and finally performing vacuum dehydration to proper viscosity at the temperature of 60 ℃; wherein, the mole percentage of sodium hydroxide and phenol in the sodium hydroxide aqueous solution is 0.05: 1, the molar ratio of formaldehyde to phenol is 1.7: 1;
the expandable graphite is treated by:
1) mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with expandable graphite, and drying at 55 ℃ for 6 hours for later use;
2) mixing the dried 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in the step 1) with a silane coupling agent, and stirring in an oil bath for 4 hours at the temperature of 160 ℃;
3) mixing the expandable graphite dried in the step 1) with deionized water, adjusting the pH value to 4, adding the product obtained in the step 2) and ethanol, stirring for 4 hours at the water bath temperature of 60 ℃, carrying out suction filtration and washing on the product, and drying for 5 hours at the temperature of 60 ℃;
in the present example, the length of the aromatic polyamide fiber was 9 mm.
EXAMPLE six
The component A comprises the following raw materials in parts by weight: 20 parts of composite resin, 6 parts of aromatic polyamide fiber, 2 parts of polyvinylpyrrolidone, 2 parts of ethylene glycol, 7 parts of composite flame retardant, 5 parts of triethylene diamine, 12 parts of dichloromethane, 7 parts of composite foam stabilizer and 0.8 part of polymethyl methacrylate;
the preparation method of the expandable phenolic resin comprises the following steps: mixing phenol and 37 mass percent formaldehyde aqueous solution, heating to 40 ℃, slowly dripping 50 mass percent sodium hydroxide aqueous solution into the system under rapid stirring, controlling the temperature of the system to be not higher than 60 ℃, adjusting the water bath temperature to 50 ℃ after finishing dripping, reacting for 1-3 hours, then heating to 80 ℃ for reacting for 3 hours, after the reaction is finished, rapidly cooling the system to below 40 ℃ by using cold water, adjusting the system to be neutral, and finally dehydrating in vacuum to proper viscosity at the temperature of 57 ℃; wherein, the mole percentage of sodium hydroxide and phenol in the sodium hydroxide aqueous solution is 0.05: 1, the molar ratio of formaldehyde to phenol is 1.7: 1;
the expandable graphite is treated by:
1) mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with expandable graphite, and drying at 60 ℃ for 5.5 hours for later use;
2) mixing the dried 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in the step 1) with a silane coupling agent, and stirring in an oil bath for 4 hours at the temperature of 160 ℃;
3) mixing the expandable graphite dried in the step 1) with deionized water, adjusting the pH value to 4, adding the product obtained in the step 2) and ethanol, stirring for 4 hours at the water bath temperature of 60 ℃, carrying out suction filtration and washing on the product, and drying for 5.5 hours at the temperature of 60 ℃;
in the present example, the length of the aromatic polyamide fiber was 8 mm.
In the above embodiment, the composite resin is an expandable phenolic resin and a urea-formaldehyde resin in a mass ratio of 2: 1, compounding; the composite flame retardant is prepared from dimethyl methyl phosphate: tris (1-chloro-2-propyl) phosphate: expanded graphite 12: 8: 15, compounding; the composite foam stabilizer is castor oil polyoxyethylene ether in mass ratio: tween-80 ═ 3: 1, compounding; the composite curing agent is benzene sulfonic acid: dimethylolpropionic acid ═ 2: 1, compounding.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (8)
1. A method for sealing a remote fire area in a coal mine well is characterized by comprising the following steps: the method comprises the following steps: a. performing directional drilling construction from an air inlet roadway and an air return roadway of a ground fire zone working face by using an accurate positioning drilling technology, and determining a construction position of a fire zone sealing wall;
b. respectively filling polymer filling materials into the drill holes of the air inlet lane and the air return lane through pipelines to form a sealing wall;
the polymer filling material comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 15-25 parts of composite resin, 4-8 parts of aromatic polyamide fiber, 1-3 parts of polyvinylpyrrolidone, 1-3 parts of ethylene glycol, 5-10 parts of composite flame retardant, 3-7 parts of triethylene diamine, 10-15 parts of dichloromethane, 5-10 parts of composite foam stabilizer and 0.5-1 part of polymethyl methacrylate;
the composite resin is prepared from expandable phenolic resin and urea-formaldehyde resin according to the mass ratio of 2: 1, compounding; the composite flame retardant is prepared from dimethyl methyl phosphate: phosphoric acid triester: expanded graphite 12: 8: 15, compounding; the composite foam stabilizer is castor oil polyoxyethylene ether in mass ratio: tween-80 ═ 3: 1, compounding;
the component B comprises benzene sulfonic acid in a mass ratio: dimethylolpropionic acid ═ 2: 1, compounding.
2. The method for closing the remote fire area in the underground coal mine according to claim 1, which is characterized in that: and in the step b, inputting nitrogen as conveying power during filling and monitoring pressure.
3. The method for closing the remote fire area in the underground coal mine according to claim 2, which is characterized in that: in the step B, the component A and the component B are conveyed to the bottom of a drilled hole according to the ratio of 4: 1-8: 1 and then mixed by a static mixer.
4. The method for closing the remote fire area in the underground coal mine according to claim 1, which is characterized in that: the pipeline includes A group's component conveying line and B group's component conveying line and communicates the imported nitrogen gas auxiliary line who communicates A group's component conveying line import and B group's component conveying line import respectively, be provided with the manometer on the nitrogen gas pipeline, be provided with flowmeter and flow control valve and check valve on A group's component conveying line and the B group's component conveying line.
5. The method for closing the remote fire area in the underground coal mine according to claim 1, which is characterized in that: the outlets of the component A conveying pipeline and the component B conveying pipeline are arranged within 20cm of the top plate of the closed roadway.
6. The method for closing the remote fire area in the underground coal mine according to claim 1, which is characterized in that: the preparation method of the expandable phenolic resin comprises the following steps: mixing phenol and 37 mass percent formaldehyde aqueous solution, heating to 35-45 ℃, slowly dripping 50 mass percent sodium hydroxide aqueous solution into the system under rapid stirring, controlling the temperature of the system to be not higher than 60 ℃, adjusting the water bath temperature to 45-55 ℃ after finishing dripping, reacting for 1-3 hours, then heating to 75-85 ℃ for reacting for 2-4 hours, after the reaction is finished, rapidly cooling the system to below 40 ℃ by cold water, adjusting the system to be neutral, and finally performing vacuum dehydration to proper viscosity at the temperature of 55-60 ℃.
7. The method for closing the remote fire area in the underground coal mine according to claim 6, wherein the method comprises the following steps: the mole percentage of sodium hydroxide to phenol in the sodium hydroxide aqueous solution is 0.05: 1, the molar ratio of formaldehyde to phenol is 1.6-1.8: 1.
8. the method for closing the remote fire area in the underground coal mine according to claim 1, which is characterized in that: the expanded graphite is treated by:
1) mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with expanded graphite, and drying at 55-65 ℃ for 5-6 hours for later use;
2) mixing the dried 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in the step 1) with a silane coupling agent, and stirring in an oil bath at the temperature of 150-;
3) mixing the expanded graphite dried in the step 1) with deionized water, adjusting the pH value to 3-5, adding the product obtained in the step 2) and ethanol, stirring for 3.5-4.5 hours at the water bath temperature of 55-65 ℃, filtering, washing and drying the product at the temperature of 55-65 ℃ for 5-6 hours.
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| CN101663374A (en) * | 2007-04-03 | 2010-03-03 | 巴斯夫欧洲公司 | DOPO flame retardant compositions |
| CN103788325A (en) * | 2014-01-24 | 2014-05-14 | 胡相明 | Reinforced efficient, inflaming retarding and antistatic composite material for mining |
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